Distillation apparatus



July 21, 1942. H. ROSENTHAL 2,290,209

DI S 'I'ILLAT ION APPARATUS Filed March 18, 1939 s Sheets-Sheet 1 Z FIGURE 2 FIGURE y 1942- H. ROSENTHAL 2,296,209

DISTILLATIONFAPPARATUS Filed March 18, 1939 3 Sheets-Sheet 2 FIGURE 3 FIGURE 4 July 21, 1942. ROSENTHAL 2,290,209

DISTILLATIONYAPPARATUS Filed March 18-, 1939 3 Sheets-SheetS FIGURE 6 FIGURE 7 1 T FlGURE 5 Patented July 21, 1942 sTATEs PATENT, OFFICE 2,290,209 wah e 'ama DISTILLATION APPARATUS Henry Rosenthal, Yonkers, N. Y. App ication March-18, 1939, Serial No. 262,713

. extraction of cottonseeds with propane, that if Claims. My invention relates to a novel still, suitable tor separating a solution having a relatively volatile and a relatively non-volatile compo- Aug. 4, 1934, for Oil treating process, Pat. No.

2,152,664; Serial 738,400, filed Aug. 4, 1934, for Oil extraction, Pat. No. 2,152,665; and Serial 218,068, filed July 8, 1938, for Petroleum oil refining.

In Serial 738,399 there is claimed a novel method of extraction anda novel form of extractor; in, Serial 738,400, there is claimed a novel method of extraction and a novel form of extractor; in

the heat be applied substantially continuously throughout the still, the major portion of the propane may be removed from the solution without subjecting the oil to maximum temperatures for appreciable periods. results in oil of a higher quality than is obtained when the heat is applied for alonger time. Moreover, in the removal of the initial propane, it desirable to maintain relatively high pressures in the still in order that the major portion of the propane may be evaporated and the vapors condensed without the need of compressing vapors or gases, as this results in an economy of operation.- The heating surfaces must thus be designed to withstand the pressures involved. Moreover, the propane va- Serial 218,068 there is claimed a novel method of refining petroleum.

Where it is desired to separate two components volatile, by distillation of the volatile component from the solution, the use of'a fractionating column and reflux condenser is not necessary for obtaining a good separation of the components. This is particularly the case where the relatively non-volatile component is the desired 'fraction and the volatile component is condensed and the condensate utilized as solvent in preparing an additional quantity of solution. for separation.

Where there is sufiicient difierence between the boiling points of the two components, substanpors released near the bottom of the column will be at a higher temperature than either the vapors released near the top of the column or with the liquid solution entering the column, and will in fact be superheated in respect to the propane liquid in the condenser. By providing heat exchange'between these superheated vapors and liquid solution rich in propane, the superheat is removed in evaporating more propane rather than being carried into the condenser and interfering with the operation of the condenser. Furthermore, I find by heating the solution in relatively thin sheets .01 layers with a large. vapor of a solution, one of which components is relag releasingsurfacerthat not only is the tendency tively volatile and the othefrelatively norr to prime or foam reduced, but also that local tially none 01. the less volatile component will The use of a reflux condenser, moreover, does not add to the quality of the less volatile component withdrawn from the bottom of-the still unless the temperature and pressure conditions at the bottom of the still are such that an appreciable portion of the less volatile component is, vaporizedunder these conditions.; 0n the other hand, theapplication of all heat at the bottom 0'! the column for the vaporization of the more volatile component, causes the less volatile component, to be subjected to maximum temperatures for an appreciable. period.

I have found, for example in the separation of propane from the oil solution formed in .the

overheating of the solution isavoided. All of these advantages, 1 provide in my novel still.

In the distilling'operation, the frgghidlution--- entering the still and colitai'fifn g a'large portion of the more volatile component will have an appreciably lower boilingpoint than doesthe solution after a portion of the more volatile component has been removed. 'lihe boiling point of the solution thus progressivelyincreases until the maximum amount of the more volatile compo-r or any other heat of low'temperature. Where the solution is delivered tov the top of the still and allowed to flow by gravity to the bottom of thestill, this low grade heat may be used in the ,top sections of the still where most of the evap oration of the more volatile component will take place, and high grade heat will beneeded only z in small amounts in-the lower sections.

a The vapors from anysection are superheated withrespect ,to the solution in the. next higher section, and it this vapor is madeto pass through the liquid insuch next higher section, then the supply heat progressively.

The objects of my invention are thus to provide a still in which- Y 1. The maximum temperature is applied to the solution for a minimum period.

2. High pressures may be maintained within the still.

3. Heat is applied to the solution progressively.

'inHeat exchange is provided between the out- 20 going vapors and the incoming solution.

5. Heat is applied to .the solution while the solution is in relatively thin layers.

6. Large vapor releasing surfaces are provided.

7. Low grade heat may be used in part of the still and high grade heat may be used in another portion of the still.

Other objects of my invention will be apparent from this specification.

My invention maybe best understood by reference to the accompanying drawings which form a part of this specification, and in which Figure 1 shows a cross section of one form of my still in which the heating elements are formed of flanged and dished heads.

Figure 2 shows an enlarged view of the heating and distributing elements of the still of Figure 1.

Figure 3 shows an elevation of a modified form of still of three pressure sections, in a single assembly.

Figure 4 shows an enlarged vertical section'of the still of Figure 3.

Figure 5 shows an elevation of a form of still, suitable for relatively large through-puts, and in which the heating medium may be supplied at a plurality of temperatures in a single pressure stage.

Figure 6 shows an enlarged horizontal section on plane 6-6 of Figure 5.

Figure 7 shows an enlarged verticalsection on the plane 'I-l of Figure 6. a

Figure 8 shows an enlarged vertical section on the plane 8-8 of Figure 6.

Now referring to Figures 1 and 2, the still I is a substantially vertical pressure vessel with the cylindrical shell ii, the bottom head lifand the top head l1. Solution is delivered to. the upper portion of still I by means of the pipe I4, and vapor is discharged to condenser H0 by pipe 21.

Still I contains a plurality of heated trays, with alternate distributing sections shown in greater detail in Fig. 2.. Steam or other fluid may be used as heating medium. The solution enters the upper distributing section Ida and is (118- charged at the circumference over the serrated upturned vertical circumferential edge a. The solution thus discharged irom the distributing section "a is delivered around the circumference of the heated tray 20a. The solution drains to the center of this tray and is discharged by the nipple 21c into the second dish'ibutiis e tion 18b and continues in a like manner it reaches the bottom of the still. In: its e over the heated trays, solvent is evaporated and the temperature of the solution increases ma concentration increases in its passage downward. The solution is heated only so long as it is in contact with the heated trays. Its time of contact with the heating means is therefore of relatively short duration. Furthermore, the heating is done with the solution in thin flowing him. This has two advantages:

1. It prevents overheating, as the solution in thin fllms will tend to uniformly maintain the temperature corresponding with the pressure in the still and the concentration of the solution at the instant.

2. 'Iheuseofthethinfilmstendstolimltany priming or foaming. Priming or foaming is not to be expected in the upper portion of the still where there'is a relatively large fraction of the more volatile component. Any bubbles formed in the lower portion of the still will tend to be broken up before they reach the vapor outlet 22.

f The concentrated less volatile component from the lowest heating tray I812. is discharged to a pool 23 at the bottom of the still where it i out of contact with further heat. The level of this pool 23 is controlled by the level control valve 24, inpipe II, which maintains proper level in the pool by opening-when a predetermined upper level is reached and closing when a predetermined lower level is reached. The amount of heating of the solution is controlled by the thermostatic valve. 26, which admits heating medium to the upper tray 2M, through the pipe It. This thermostatic valve is controlled by the thermostat 26 in the pool 23.

The material entering the still at the upper distributing section l8a will have a relatively large amount of the more volatile component of low boiling point. The vapor tension and vapor pressure of this solution at any temperature time depend upon the mm per cent of the less volatile component and more volatile component in the solution, and the temperature of the solution. At any particular temperature, then, the vapor pressure and vapor tension will be at a maximum for the maximum mol per cent or the less volatile component.

Conversely, if the pressure is substantially fixed, as it is in the interior of still I, the temperature of the solution is a minimum with the maximum concentration of the more volatile component. 7 Thus any attempt to add an increment of heat to the solution results primarily in vaporizing a portion or the solution. Thus the increment of heat so added appears largely as latent heat of vaporization and does not act to raise the temperature of the solution except as the vaporization acts to increase the concentration of the less volatile component in the solu- As the concentration of the less volatile component increases progressively as the solution passes down the still and as the maximum concentratlon' of the less volatile component is at the bottom of the still, the maximum temperature of the solution within the still will be at this locatlon. Accordingly, I place the control of the heating medium at this location in order to accurately limit the mairimum temperature not the solution. 7

Each heating tray 2|, in order to easily withstand the pressures within the still, is composed of two dished/heads lointed together by any suitable means such as welding, forming togetherachamberflasshowninflsurezinto which the heating medium is admitted. The

. Ill.

tinues down the still until it is discharged through pipe 29. a

The pressure in still I is controlled by the direct connection of the still I to condenser H3,

and will depend upon the vapor pressure of the less volatile component at the temperature of the vapors in the condenser. In this manner. all of the vapors generatedin still I may be condensed without compression. However, the pressure that will be generated within the still will limit the v amount of the evaporation that will take place in the still, so that the solution discharged through pipe l2 will contain measdensate bypipe I I4. The flow of steam is shown as controlled by valve H5 which is regulated by thermostat H6 in the liquid at the bottom of the still as it is about to be discharged through pipe The level of liquid in the still is controlled by valve H8 operated by-the liquid level controller H9. The temperature of still I is preferably controlled at the same value by thermostat H6 as that maintained in still i under the control of thermostat 26.

Vapor leaves the still through pipe I20 and is delivered to compressor I2I which maintains any desired pressure in the still ill' below that of still I. Where still III is depended upon to eliminate the final traces of the less volatile component, I prefer that a high vacuum be maintained in still Ill. Compressor l-2l compresses the vapors from still Ill and delivers them to pipe I22 which may lead to condenser H0.

Still IH may be replaced with a plurality of stills to provide more than two pressure stages, and in Figures 3 and 4 I illustrate such arrangement.

In describing Figures 1 and 2, I have explained the operation of a simple form of my invention, and in which two pressure stages are shown. In some applications, a greater number of pressure stages is preferable for removing the more volatile fraction substantially completely from the solution. A still with three pressure stages contained in a single shell is shown in Figures 3 and 4.

Referring to these two figures, the still 30 is a substantially vertical cylindrical member having the shell 3|, the bottom head 32..the top head 33 and the intermediate heads 34, 35, and 36. As shown, the section 43 between the bottom head 32 and the intermediate head is for an elevated pressure above atmosphere; the section 4| between the intermediate heads 36 and in order to prevent the vapors leaving sectionll from being' superheated by contact with the metal of head 36, which will be at substantially the same temperature as the liquid in section 4| and thus appreciably hotter than the vapors from section 43f 1 Solution enters the pipe I4 onto distributer plate 2', and overflows the serrated circumferential lip 3 of the plate, and falls in the form of atrain onto the distributer plate 4. .The solution on distributer plate 4 overflows-theserrated circumferential lip 5 of the plate and falls in the form of a rain onto the heating tray 43a. The cylindrical closed cover, 6 is shown placed above the trays 2 and 4 in such a manner that the vapors leaving the still'thru pipe 22 are forced to pass through the rain of solution as it falls from each of the trays as described above.

The solution falling on heating tray 43a flows down the tray over the heating surface and passes through thepipe nipple 44 onto the heating tray 43b, over which it passes upwardly and overflows the circumference of the trayonto' the heating tray 430.. The solution flows down tray 43c and passes through the pipe nipple 45 onto distributer tray 50. It overflows the upper serrated edge-of the distributer tray 50 and falls'in the form of a rain from the lower serrated edge of the tray onto the distributer tray T. I-have shown three heating trays 43a, 43b, and 430, in the upper portion of the high pre'ssuresection 40. It will be understood, however, that a greater or less number may be used as desired. In the form shown, both sides of each of the heating trays are used as heating surfaces, and the solution is held in a relatively thin'sheet by proper spacing of the trays in respect to each other. The hollow member 46, placed above the-upper tray 43a, prevents the solution from remaining on the tray 43a in the form of adeep pool. This hollow member may also be used for heating surface where desired, but I prefer generally that the hollow member be unheated in order to prevent superheating of the vapors'which pass over the upper surface of the member 43 and through pipe nipple 39 on their way tothe vapor outlet pipe 22. As shown, the hollow'member 46, and the heating trays 43a, 43b, and 430, are formed from flanged and dished heads united with each other in any suitable manner, as for instance, by welding. Heating medium,

trays through the pipe l3, and steam and condensate passes through nipples 41, 43, and 49 in-- to outlet pipe 59. Pipe 52, suitably connected to each of the heating trays, serves for removin air or other non-condensable gases from the interior or the trays, and thus to provide for" free circulation of steam to the trays.

36 is for a pressure about that of the atmos- Solution falling iromtheupper portion of the high pressure section 46 onto the distributer tray 1 overflows the upper serrated edge of the distributer tray and falls in the form of a rain onto the heating tray'63a below. All vapors'generated in section 43 below the distributer tray I are forced to pass through this rain and to enter into heat exchange with the falling solution. The

withheating medium through the pipe 6|, and

pipe 32 serves to vent the non-condensable gases assteam, enters the hollow interior of the heating falls into the pool 31 provided with heating coils from these trays. Pipes 5?, 58, and 59 provide for removal of condensate to the pipe 6!.

I have shown only two portions in section 40, but as many portions may be provided as are desired, each of the lower portions comprising an upper distributer tray such as tray I, heating trays with their connections for heating medium such as trays 53a, 53b, and 530, and a lower distributer tray such as tray 60. For a bottom portion, the tray 60 willdischarge into the pool 23 at the bottom of the column. For an intermediate portion, the tray 60 will discharge into a distributer tray in the same manner that tray 50 discharges into tray I.

Vent pipes 52 and 62 are shown as discharging into the header pipe 8. Pipe 6| from the heating trays of the bottom poltion also discharges into this header. At the bottom of the header, 2. suitable trap such as shown at 9, is provided to prevent loss of steam through the condensate pipe GI. At the top of the header, a suitable valve 63 is provided to prevent loss of steam with the vented non-condensable gases. A small condenser 64 may be provided in line 8 ahead of valve 63. from the pool 23 at the bottom of section 40.

The amount of the more volatile material remaining in the solution in pool 23 will depend upon the limitations of temperature that must be imposed to prevent deterioration of the less volatile component. Where my still is used in connection with the separation of a propane and crude cottonseed oil solution such as is obtained in the solvent extraction of dottonseeds with propane, I prefer that the maximum temperature to which the oil is heated be of the order of 200 F., in which event the propane will comprise about 4% of the weight of the solution in pool 23, when the pressure maintained in the section is suficient to condense the propane with a temperature of condensing water such as is commonly encountered. In order to remove the remaining portions of the propane, the solution is treated under lower pressure conditions. Thus, the solution removed through pipe I2 may be introduced into a stillrsection II maintained at about atmospheric pressure. Here the propane content may be reduced to a fraction of one per cent of the solution without exceeding temperature limitations. Still section 4| may be similar to section 40 just described, but in the present example, the'portion of the more volatile component is so small that relatively little heat need be provided for its vaporization. Thus as shown, the solution from pipe I2 enters section 4| into a series of distributer trays 65 from which it 68 supplied with steam through the pipe 61. As shown, a rotary foam breaker I00 is provided in thestill above the pool 31.. Vapors released from the solution are conducted through the rain of solution provided on the serrated distributer trays 65, before being conducted from the section AI.

Solution from the pool 31 is discharged through pipe 66 to section 42, maintained under high vacuum. Here the last traces of the more volatile component are removed. As shown, the solution enters on a series of distributing trays IIII, similar to the trays 65 of section II. From these trays the solution falls as a rain into the pool I02, provided with the open steam coil I03, and the mechanical agitator I04. Above the pool is the mechanical foam breaker I05. Vapors of sol vent and steam leave section 42 by pipe I01 after coming in heat exchange with the incoming solu- Pipe I2 serves for removing solution tion at the distributer section MI. The propane free oil is withdrawn from pool I02 by pipe I06.

While I have not shown thermostatic control of the heating medium in Figures 3 and 4, in order that the drawings be not needlessly complicated, I prefer that such thermostatic control he applied in the same manner as is illustrated in Figure 1; and that substantially the same maximum temperature be maintained in each of the sections of the still I, by means of a separate thermostat in each section, each of the separate thermostats controlling the heating medium to that section of the still corresponding with the location of the particular thermostat. In placing the thermostat in each section, it should be preferably placed in the hottest location in the section, as, for instance, in the pool at the bottom of the section.

Now, referring to Figures 5, 6, 7, and 8, I have shown a modified form of still, applicable to treating relatively large quantities of solution, and particularly adaptable for use where higher temperatures may be utilized, as for instance in separating propane from lubricating oil. This modification is provided with two temperature stages of heating in a single pressure stage, which pressure'stage may correspond with the stage of section 40 of Figures 3 and 4, or with still I of Figure 1.

In Figures 5, 6, '7 and 8, the still I6 is shown as a closed, vertical, cylindrical pressure Vessel, having the metallic cylindrical shell I0. shell is provided with a series of rings attached to the shell, the rings having a 2 section as shown at H. These rings serve for mounting a series of alternate trays I2 and I3, trays "I2 being distributer trays and trays I3 being heating trays. I prefer-that each of these trays be made sectional so that it may be brought through a convenient manhole in the shell I0, so that the trays can be formed on the interior of the shell merely by hanging the inverted L-shaped lip I4 of the sections over the upstanding flange of the 2 rings II The trays may thus be built up, starting at the bottom tray and continuing to the top. The heating pipe connections I5 and IE to each heating tray may be made up tight before the next superimposed distributer tray is placed in position.

Each distributer tray I2 completely covers the central portion of the still as shown in the sectional elevations, Figures 7 and 8. At each edge the distributer tray terminates in an overflow weir I! having serrated edges. Solution entering the distributer tray either from the feed line I9 at the top or from a superposed heating tray below the top, overflows the weir TI and drips as a fine rain-80, from the serrated lower edge of the weir I1.

This rain falls in the pools 8I of the heating tray immediately below. From the pools 8i, the solution is conducted by the batlles 82, over the heating coils 84, where the solution is heated in relatively thin sheets. The path of the solution past the coils is shown by the solid arrows of Figure 6. Each heating coil comprises the tubes 84 secured in the headers 85. After leaving the heating coils, the solution enters the pool 89 from which it overflows the serrated circular weir 81 and drips as a fine rain 90 from the serrated lower edge of the weir 81.

This rain 81 falls into the pool SI of the distributer tray immediately below, from which the solution falls over the weir II as described above.

In this manner, the solution continues down the This tower until it enters the pool 92 at the base of the tower, from which it is discharged through valve l8 operated by the level control mechanism l9.

As will be noted, particularly in Figure 8, all the vapors generated on any of the heating trays below any particular distributer tray must pass still will be determined largely by the concentration of the solution at that point. As the amount of solvent in solution decreases progressively downward through the still, the temperature of the solution increases progressively as the solution passes downward through the still; Thus, the vapors released on a lower heating tray will be superheated with respect to'the liquid on the heating tray next above, or any of the other heating trays above. But as this superheated vapor is forced into intimate contact with the descending liquid, the superheat is used ,up in evaporating an additional amount of solvent.

Relatively low temperatures are required to evaporate the bulk of the propane from the solution, so that low pressure steam entering through pipe 94 and discharging as condensate through trap 95, may be used as heating medium for the coils in the upper heating trays. For the bottom heating trays, a high temperature vapor is preferably used as the heating medium, entering through pipe 96 and discharging through It will be apparent thatwhile I have used propane solutions in the examples which I have used for the illustration of my invention, other solutions may readily be treated in a like manner. Moreover, in. the illustrations, I have referred to the heating medium as steam, but other heating media may be used as best suits the particular application. Thus, hot water or vapors of a low boiling liquid may be used in the closed coils where low temperature heat is desired; or hot oil, or the vapors of a high boiling compound as diphenyl, diphenyl oxide, mercury, etc., may be from the still, and means for conducting heating medium to and from the heating trays.

2. In a system or distillation, a closed, vertical pressure vessel havingran inlet forsolution and an outlet for solvent vapors both disposed near the top of the vessel; an outlet for solute disposed near the bottom of the vessel; and a plurality of alternate serrated heating trays and serrated distributing trays arranged so that the passages by the heating trays are staggered with relation to the passages by the distributing tray and that external heat may be applied to the solution progressively as the solution passes downwardly through the vessel, and that vapors generated on a lower heating tray are passed thru the solution descending from the serrations of a superimposed heating tray.

3. In a system of distillation, a closed, vertical pressure vessel having an inlet for solution, an outlet for solvent vapors, and an outlet for liquid solute; heating means disposed progressively within said pressure vessel to progressively apply heat to and raise the temperature of the solution; and bafiie means provided with serrations adapted to comminute the descending liquid disposed between the heating means; and passages bythe heating means staggered in relation to the passages by the baflle'means to conduct as- I cending vapors through a comminuted stream of descending solution, descending from the serrations of the bailie means.

4. In a system of distillation, a closed, vertical the solution is flowing in relatively close proximity used where high temperature heat is desired.

Also, it will be apparent that many other changes may be made in my invention without departing from the scope of the invention as defined in the appended claims.

Now having described my invention in a manner that it may be readily understood by one skilled in the art, I claim:

1. In a system of distillation, a closed still for the continuous separation of solvent from a solution, said still comprising a vertical closed cylinto said heating means and as said solution progresses from the top to the bottom of said vessel, distributing means provided with serrations adapted to comminute the descending liquid disposed alternately with said heating means, and openings in said heating means and distributing means so placed relative to each other that the passages by the heating 'means are staggered relative to the passages by the distributing means and that the vapors generated by a lower heat-- ing means are passed through the solution de scending from the serrations of a superimposed distributing means. i

5. In a system of distillati n, a closed, vertical vessel having an inlet for sdlution and an outlet for vapors both disposed near the .topof the vessel; an outlet for liquid disposed near the bottom of the vessel; means for applying external heat progressively to the solution while the solution is flowing in relatively close proximity to said heating means and as said solution progresses from the top to the bottom of said vessel, whereby the temperature of the solution is progressively increased from the top to' the bottom of said vessel, said means for applying heat being provided with serrated overflow means for said solution; distributing means disposed alternately with said heating means: and openings in said heating means and distributing means so placed relative to each other that the passages by the heating means are staggered relative to the passages by the distributing means and that the vapors generated by a lower heating, means are passed through the solution descending from the serrations of a superimposed heatinglneans.

HENRY 

